EP0332738B1 - Verfahren zur Reduktion des Alkoholgehaltes von alkoholischen Getränken - Google Patents

Verfahren zur Reduktion des Alkoholgehaltes von alkoholischen Getränken Download PDF

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Publication number
EP0332738B1
EP0332738B1 EP88116674A EP88116674A EP0332738B1 EP 0332738 B1 EP0332738 B1 EP 0332738B1 EP 88116674 A EP88116674 A EP 88116674A EP 88116674 A EP88116674 A EP 88116674A EP 0332738 B1 EP0332738 B1 EP 0332738B1
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EP
European Patent Office
Prior art keywords
alcohol
membrane
condensation
permeate
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP88116674A
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German (de)
English (en)
French (fr)
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EP0332738A1 (de
Inventor
Hartmut Ernst Arthur Dr. Brüschke
Walter Schneider
Günter F. Tusel
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Deutsche Carbone AG
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Deutsche Carbone AG
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Publication date
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Publication of EP0332738A1 publication Critical patent/EP0332738A1/de
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
    • B01D61/362—Pervaporation
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H3/00—Methods for reducing the alcohol content of fermented solutions or alcoholic beverage to obtain low alcohol or non-alcoholic beverages
    • C12H3/04—Methods for reducing the alcohol content of fermented solutions or alcoholic beverage to obtain low alcohol or non-alcoholic beverages using semi-permeable membranes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S159/00—Concentrating evaporators
    • Y10S159/27—Micropores

Definitions

  • the invention relates to a method for reducing the alcohol content of alcoholic beverages, in particular beer and wine, by means of pervaporation.
  • ethanol can be distilled off from alcoholic beverages, such as wine or beer, thereby reducing the ethanol content of the beverage.
  • alcoholic beverages such as wine or beer
  • Such a method is e.g. B. for beer in brewery industry 71 (1986), page 480.
  • the distillation In order to protect heat-sensitive components in beer, the distillation must be carried out at a low temperature and therefore under reduced pressure. Under these conditions, apart from ethanol, other substances which are essential for the taste are removed from the beer in accordance with their volatility, so that taste impairment cannot be avoided.
  • protein components are denatured at the required temperatures, which also leads to changes in the taste and appearance of the low-alcohol beer.
  • the distillation process under reduced pressure also removes the free carbonic acid from the beer, which then has to be recompressed and added again. The technical effort and the costs for such a vacuum distillation are high, without which this ultimately leads to a satisfactory result.
  • a disadvantage of this process is also the fact that under the action of the required high pressure, a denaturation of flavors occurs, and that in addition to alcohol and water, other flavors also pass through the membrane and are therefore lost. Further an alcoholic solution of low concentration is obtained as permeate, which has to be processed or disposed of. Despite the disadvantages described, this process of reverse osmosis is used on an industrial scale, which clearly shows the need for better processes.
  • DE OS 36 10 011 describes a process for the absoluteization of alcohol by means of pervaporation, the permeate being subjected to a fractional condensation and low-concentration and higher-concentration alcohol being obtained in the process.
  • the lower-concentration alcohol is fed back into a first pervaporation stage, while the higher-concentrated alcohol is absolute in a second pervaporation stage.
  • the invention now relates to a method for reducing the alcohol content of alcoholic beverages according to claim 1.
  • the original alcoholic beverage e.g. B. beer or wine
  • fed to the inlet side of a pervaporation membrane A two-stage condensation of the permeate takes place on the permeate side, a main condensation being followed by a post-condensation, the post-condensation in turn being multi-stage.
  • the main condensation works with pressures from 0.5 to 50 mbar and temperatures from 0 to -30 ° C, while the post-condensation takes place at stepped higher pressures than the main condensation up to atmospheric pressure and at temperatures from -20 to -70 ° C, this temperature being lower than the main condensation temperature. It has been found that the volatile aroma substances contained in the alcoholic beverage permeate through the membrane.
  • the separated alcohol is obtained in the main condensate in a concentration that is significantly higher than the concentration in the original alcoholic beverage. This gives a directly usable product as permeate, which can also be easily concentrated to pure alcohol.
  • the process of the invention is generally carried out at feed temperatures of 0 to 80 ° C., preferably 20 to 45 ° C., temperatures of 30 to 40 ° C. being particularly preferred.
  • the process is carried out either at atmospheric pressure or slightly increased pressure on the feed side. The latter is particularly recommended for carbonated beverages, such as beer, to prevent the free carbon dioxide from escaping.
  • Typical process pressures for the feed side are in the range of 1 to 5 bar. At higher pressures, tightness problems can occur.
  • pervaporation membranes are suitable which have a higher permeability for alcohol (ethanol) than for water.
  • a preferred group of membranes are those made from silicones, in particular from polydimethylsiloxane. Polydimethylsiloxanes which, in addition to methyl groups, are also larger and / or partially or preferred contain perfluorinated alkyl or aryl substituents as side chains bound to silicon atoms.
  • Another preferred class of membranes is described in EP-A-0 254 758. These are membranes made from mixtures of hydrophobic inorganic substances such as silicalites and polysiloxanes.
  • Membranes with ion-exchanging properties, e.g. B. anion-exchange membranes are suitable for carrying out the method according to the invention.
  • pervaporation membranes are used in the form of so-called membrane modules.
  • module here denotes the structural unit consisting of the actual membrane and its holding device.
  • Suitable membrane modules are e.g. B. described in EP-A-0 214 496.
  • other membrane modules e.g. B. tubular membrane modules or spiral winding modules are known.
  • the implementation of the method of the invention is described below with reference to the drawing for beer.
  • the single figure shows a pervaporation device with membrane module 5, preheating device 2, main condenser 8, post condenser 14 and vacuum pump 12.
  • the membrane module 5 contains a pervaporation membrane 4 made of polydimethylsiloxane, which contains about 70 percent by weight of a hydrophobic zeolite (silicalite). Further process parameters are described in Example 3.
  • the permeate is discharged via line 7 and enters a main condenser 8, which is cooled via a cooling line 9 and is connected via a line 11 to a vacuum pump 12 and a further line 13 to a post-condenser 14 (single-stage post-condensation).
  • the main condenser 8 condenses the main amount of the permeate which is discharged via a line 10.
  • the vacuum pump 12 generates the desired negative pressure of 15 mbar in the main condenser 8.
  • the post-condenser 14 is cooled via a cooling line 15, is connected to the atmosphere via a line 16 and works thus at atmospheric pressure.
  • the post-condensate is discharged via a line 17.
  • the ratio of the amounts of condensate obtained in the main and secondary condensers 8 and 14 is approximately 200: 8.
  • a retentate contains a low-alcohol product which is discharged via a line 6 and has an alcohol content of only 1.7 percent by weight.
  • the post-condensate discharged from the post-condenser 14 via line 16 is added to this product, which is a volatile aroma of beer which contributes to the typical desired beer taste. This is followed by redilution with pure water to the original volume, giving the desired low-alcohol beer with an ethanol content of 1.8 percent by weight.
  • the device shown can be modified in many ways, depending on the practical circumstances. For example, in practical implementation, it makes sense to divide the entire membrane area into several membrane modules, each of which opens into the same main capacitor on the permeate side. On the retentate side, the membrane modules are linked to one another in such a way that the retentate of the previous membrane module represents the inlet for the following membrane module. If necessary, any heat losses that occur are compensated for by intermediate preheaters.
  • the post-condensation can also be carried out in a first stage under reduced pressure.
  • the line 16 of the figure is then connected to the suction side of a further vacuum pump (not shown), on the pressure side of which a further post-condenser (not shown) is optionally arranged.
  • the first post-condenser 14 then operates at a pressure between that of the main condenser 8 and atmospheric pressure.
  • the membrane is about 60 »m thick and consists of a polydimethylsiloxane, in which a part of the methyl side groups is replaced by propyl and butyl groups.
  • the membrane area is 0.45 m2.
  • the temperature on the inlet side is 30 ° C and the pressure is 1.1 bar.
  • 4.1 l of low-alcohol product are obtained as retentate with an alcohol content of 3.9 percent by weight.
  • the pressure on the permeate side is 20 mbar, the main condensation takes place at -5 ° C. In this case, 0.9 1 main condensate with an alcohol content of 38 percent by weight is initially obtained as permeate.
  • condensation is carried out on the pressure side of the vacuum pump used at ⁇ 20 ° C. under atmospheric pressure, a further 10 g of post-condensate with an alcohol content of 80 percent by weight being obtained as permeate.
  • This post-condensate obviously contains wine flavors, while the main condensate consists only of ethanol and water.
  • the alcohol content is then 3.4% by weight - this low-alcohol wine is subjected to the organoleptic test. There is no difference in taste to the original wine. Apart from ethanol and water, no other components are analytically detectable in the permeate. The permeate can thus be processed immediately for use.
  • the membrane consists of polydimethylsiloxane, which contains 70 percent by weight of a hydrophobic zeolite (silicalite).
  • the membrane is about 60 »m thick and has an area of 0.45 m2.
  • the temperature on the inlet side is 40 ° C and the pressure is 1.1 bar.
  • 4.6 l of retentate with an alcohol content of 4.2 percent by weight are obtained.
  • the condensation takes place at 20 mbar and -10 ° C.
  • a main condensate of 0.6 l with an alcohol content of 58 percent by weight is initially obtained as the permeate.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Food Science & Technology (AREA)
  • Genetics & Genomics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
EP88116674A 1988-02-11 1988-10-07 Verfahren zur Reduktion des Alkoholgehaltes von alkoholischen Getränken Expired - Lifetime EP0332738B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3804236A DE3804236A1 (de) 1988-02-11 1988-02-11 Verfahren zur reduktion des alkoholgehaltes von alkoholischen getraenken
DE3804236 1988-02-11

Publications (2)

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EP0332738A1 EP0332738A1 (de) 1989-09-20
EP0332738B1 true EP0332738B1 (de) 1994-07-06

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EP88116674A Expired - Lifetime EP0332738B1 (de) 1988-02-11 1988-10-07 Verfahren zur Reduktion des Alkoholgehaltes von alkoholischen Getränken

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US (1) US5385647A (enrdf_load_stackoverflow)
EP (1) EP0332738B1 (enrdf_load_stackoverflow)
JP (1) JPH025849A (enrdf_load_stackoverflow)
AT (1) ATE108200T1 (enrdf_load_stackoverflow)
DE (2) DE3804236A1 (enrdf_load_stackoverflow)

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JP6100042B2 (ja) * 2013-03-15 2017-03-22 三井造船株式会社 エタノール濃度低減清酒の製造方法及び製造システム
JP6100041B2 (ja) * 2013-03-15 2017-03-22 三井造船株式会社 エタノール濃度低減清酒の製造方法及び製造システム
JP6104000B2 (ja) * 2013-03-15 2017-03-29 三井造船株式会社 ノンアルコールワインの製造方法及び製造システム
JP6821911B2 (ja) * 2014-10-27 2021-01-27 三菱ケミカル株式会社 アルコール飲料中のアルコール含有量の低減化方法
CN104587834A (zh) * 2015-01-27 2015-05-06 太原理工大学 一种从低浓度水溶液中分离回收高沸点有机物的装置及方法
JP6751596B2 (ja) * 2016-06-02 2020-09-09 サッポロビール株式会社 低アルコールワイン様飲料及びその製造方法
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Also Published As

Publication number Publication date
DE3804236A1 (de) 1989-08-24
JPH025849A (ja) 1990-01-10
JPH0522504B2 (enrdf_load_stackoverflow) 1993-03-29
ATE108200T1 (de) 1994-07-15
DE3804236C2 (enrdf_load_stackoverflow) 1992-07-30
EP0332738A1 (de) 1989-09-20
DE3850563D1 (de) 1994-08-11
US5385647A (en) 1995-01-31

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